NO300850B1 - Surface-modified magnesium hydroxide or aluminum hydroxide particles, their use, and highly combustible thermoplastic polyolefin - Google Patents
Surface-modified magnesium hydroxide or aluminum hydroxide particles, their use, and highly combustible thermoplastic polyolefin Download PDFInfo
- Publication number
- NO300850B1 NO300850B1 NO904734A NO904734A NO300850B1 NO 300850 B1 NO300850 B1 NO 300850B1 NO 904734 A NO904734 A NO 904734A NO 904734 A NO904734 A NO 904734A NO 300850 B1 NO300850 B1 NO 300850B1
- Authority
- NO
- Norway
- Prior art keywords
- magnesium hydroxide
- aluminum hydroxide
- hydroxide
- thermoplastic
- modified
- Prior art date
Links
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical class [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 89
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 title claims abstract description 70
- 229920002397 thermoplastic olefin Polymers 0.000 title claims abstract description 13
- 239000002245 particle Substances 0.000 title claims description 27
- 239000000945 filler Substances 0.000 claims abstract description 20
- 239000000347 magnesium hydroxide Substances 0.000 claims description 54
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 54
- 150000001875 compounds Chemical class 0.000 claims description 49
- -1 polypropylene Polymers 0.000 claims description 34
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 30
- 239000004743 Polypropylene Substances 0.000 claims description 27
- 229920001155 polypropylene Polymers 0.000 claims description 27
- 229920002943 EPDM rubber Polymers 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 24
- 229920001296 polysiloxane Polymers 0.000 claims description 17
- 229920002725 thermoplastic elastomer Polymers 0.000 claims description 11
- 229920001577 copolymer Polymers 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 9
- 229920002614 Polyether block amide Polymers 0.000 claims description 7
- 229920003245 polyoctenamer Polymers 0.000 claims description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 229920001971 elastomer Polymers 0.000 claims description 6
- 239000000806 elastomer Substances 0.000 claims description 6
- 229920001169 thermoplastic Polymers 0.000 claims description 6
- 229920001897 terpolymer Polymers 0.000 claims description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 4
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 claims description 4
- 239000003063 flame retardant Substances 0.000 claims description 4
- 239000004416 thermosoftening plastic Substances 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 229920001400 block copolymer Polymers 0.000 claims description 3
- 239000003431 cross linking reagent Substances 0.000 claims description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 229920002379 silicone rubber Polymers 0.000 claims description 3
- 239000004945 silicone rubber Substances 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 229920006147 copolyamide elastomer Polymers 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 150000004645 aluminates Chemical class 0.000 claims 1
- 229920002635 polyurethane Polymers 0.000 claims 1
- 239000004814 polyurethane Substances 0.000 claims 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims 1
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- 235000012254 magnesium hydroxide Nutrition 0.000 description 49
- 229920000642 polymer Polymers 0.000 description 34
- 239000005038 ethylene vinyl acetate Substances 0.000 description 30
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 29
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 21
- 239000012530 fluid Substances 0.000 description 19
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 17
- 229920005629 polypropylene homopolymer Polymers 0.000 description 11
- 238000001816 cooling Methods 0.000 description 8
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 8
- 239000011159 matrix material Substances 0.000 description 6
- 229920003023 plastic Polymers 0.000 description 6
- 239000004033 plastic Substances 0.000 description 6
- 239000004698 Polyethylene Substances 0.000 description 5
- 239000004793 Polystyrene Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229920000573 polyethylene Polymers 0.000 description 5
- 239000004952 Polyamide Substances 0.000 description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 235000010755 mineral Nutrition 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229920002647 polyamide Polymers 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000013256 coordination polymer Substances 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- VPRUMANMDWQMNF-UHFFFAOYSA-N phenylethane boronic acid Chemical compound OB(O)CCC1=CC=CC=C1 VPRUMANMDWQMNF-UHFFFAOYSA-N 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 3
- 229920002633 Kraton (polymer) Polymers 0.000 description 2
- 239000005639 Lauric acid Substances 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229920003020 cross-linked polyethylene Polymers 0.000 description 2
- 239000004703 cross-linked polyethylene Substances 0.000 description 2
- WDGXHWGCFUAELX-UHFFFAOYSA-J dodecanoate zirconium(4+) Chemical compound [Zr+4].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O WDGXHWGCFUAELX-UHFFFAOYSA-J 0.000 description 2
- 229910001679 gibbsite Inorganic materials 0.000 description 2
- OUHCLAKJJGMPSW-UHFFFAOYSA-L magnesium;hydrogen carbonate;hydroxide Chemical class O.[Mg+2].[O-]C([O-])=O OUHCLAKJJGMPSW-UHFFFAOYSA-L 0.000 description 2
- 150000001282 organosilanes Chemical class 0.000 description 2
- 229920002857 polybutadiene Polymers 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- PUAQLLVFLMYYJJ-UHFFFAOYSA-N 2-aminopropiophenone Chemical compound CC(N)C(=O)C1=CC=CC=C1 PUAQLLVFLMYYJJ-UHFFFAOYSA-N 0.000 description 1
- HOZMLTCHTRHKRK-UHFFFAOYSA-N 2-methyl-1-silylprop-2-en-1-one Chemical class CC(=C)C([SiH3])=O HOZMLTCHTRHKRK-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006664 bond formation reaction Methods 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 210000001217 buttock Anatomy 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000011222 crystalline ceramic Substances 0.000 description 1
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- SJYNFBVQFBRSIB-UHFFFAOYSA-N norbornadiene Chemical compound C1=CC2C=CC1C2 SJYNFBVQFBRSIB-UHFFFAOYSA-N 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920002959 polymer blend Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/02—Copolymers with acrylonitrile
- C08L9/04—Latex
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/028—Compounds containing only magnesium as metal
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S428/00—Stock material or miscellaneous articles
- Y10S428/92—Fire or heat protection feature
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S525/00—Synthetic resins or natural rubbers -- part of the class 520 series
- Y10S525/911—Polymer from ethylenic monomers only, having terminal functional group other than unsaturation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/256—Heavy metal or aluminum or compound thereof
- Y10T428/257—Iron oxide or aluminum oxide
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/258—Alkali metal or alkaline earth metal or compound thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
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- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2927—Rod, strand, filament or fiber including structurally defined particulate matter
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
- Y10T428/2998—Coated including synthetic resin or polymer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31652—Of asbestos
- Y10T428/31663—As siloxane, silicone or silane
Abstract
Description
Oppfinnelsen angår overflatemodifiserte magnesiumhydroksyd- eller aluminiumhydroksyd-partikler, anvendelse av partiklene i termoplastiske polyolefiner, samt tungt brenn-bare termoplastiske polyolefiner som inneholder overflatemodifisert magnesiumhydroksyd eller alumiumhydroksyd ifølge oppfinnelsen. The invention relates to surface-modified magnesium hydroxide or aluminum hydroxide particles, use of the particles in thermoplastic polyolefins, as well as highly flammable thermoplastic polyolefins containing surface-modified magnesium hydroxide or aluminum hydroxide according to the invention.
Ved innarbeidingen av magnesiumhydroksyd eller aluminiumhydroksyd i plaststoffer oppstår på den ene side problemet med innarbeidbarhet og forenlighet av magnesiumhydroksydet eller aluminiumhydroksydet med plaststoffet, og på den annen side må plaststoffet som er tilsatt magnesiumhydroksyd eller aluminiumhydroksyd oppfylle de nødvendige egenskaper, spesielt når det gjelder brannforhold. When incorporating magnesium hydroxide or aluminum hydroxide into plastics, on the one hand, the problem of workability and compatibility of the magnesium hydroxide or aluminum hydroxide with the plastic material arises, and on the other hand, the plastic material to which magnesium hydroxide or aluminum hydroxide has been added must meet the required properties, especially when it comes to fire conditions.
Det har derfor ikke vært mangel på innsats når det gjelder å modifisere flammehemmende fyllstoffer på en slik måte at de uten vanskeligheter kan innarbeides i plast-stoffene uten at det går ut over plaststoffenes egenskapsprofil, spesielt når det gjelder brannforhold. There has therefore been no lack of effort when it comes to modifying flame retardant fillers in such a way that they can be incorporated into the plastics without difficulty without affecting the properties profile of the plastics, especially when it comes to fire conditions.
Det er således f.eks. kjent fra DE-PS 2 659 933 at magnesiumhydroksyd kan overtrekkes med anioniske overflate-aktive stoffer, som f.eks. alkalisalter av høyere fettsyrer. Det går imidlertid tydelig frem av sammenligningsforsøkene at magnesiumhydroksyder som er modifisert på denne måte ikke tilfredsstiller de krav som stilles. It is thus e.g. known from DE-PS 2 659 933 that magnesium hydroxide can be coated with anionic surfactants, such as e.g. alkali salts of higher fatty acids. However, it is clear from the comparison tests that magnesium hydroxides which have been modified in this way do not satisfy the requirements.
Fra EP-søknad 292 233 er det videre kjent at fyllstoffer som f.eks. magnesiumhydroksyd eller aluminiumhydroksyd kan belegges med en polymer som inneholder umettede syregrupper og innarbeides i en olefin/akrylpolymer. From EP application 292 233 it is further known that fillers such as e.g. magnesium hydroxide or aluminum hydroxide can be coated with a polymer containing unsaturated acid groups and incorporated into an olefin/acrylic polymer.
Eksempelvis blir magnesiumhydroksyd eller aluminiumhydroksyd i en matrikspolymer belagt med en maleinisert poly-butadien. De likeledes som flytende elastomerer betegnede polybutadienbelegg har imidlertid på grunn av de tallrike dobbelbindinger den store ulempe at de er svært følsomme mot UV- og ozoninnflytelse, dvs. at egenskapsprofilen for det på' denne måte behandlede fyllstoff, hhv. fyllstoffet som inneholder forbindelsene, blir dårligere under påvirkning av de nevnte innflytelser. Dessuten er det på grunn av beleggets lave temperaturtoleranse satt grenser når det gjelder valg av compounderingsaggregatet ved compounderingen av et slikt modifisert fyllstoff i et plaststoff. For example, magnesium hydroxide or aluminum hydroxide in a matrix polymer is coated with a maleinized poly-butadiene. However, due to the numerous double bonds, the polybutadiene coatings also referred to as liquid elastomers have the major disadvantage that they are very sensitive to UV and ozone influence, i.e. that the property profile of the filler treated in this way, resp. the filler containing the compounds deteriorates under the influence of the aforementioned influences. Furthermore, due to the coating's low temperature tolerance, limits have been set when it comes to choosing the compounding unit when compounding such a modified filler in a plastic material.
Det oppstod således den oppgave å modifisere magnesiumhydroksyd- eller aluminiumhydroksyd-partikler på en slik måte at de ikke oppviser ulempene ifølge teknikkens stand. Denne oppgave kunne løses med ifølge oppfinnelsen overflatemodifiserte magnesiumhydroksyd- eller aluminiumhydroksyd-partikler ifølge krav 1. The task thus arose of modifying magnesium hydroxide or aluminum hydroxide particles in such a way that they do not exhibit the disadvantages according to the state of the art. This task could be solved with, according to the invention, surface-modified magnesium hydroxide or aluminum hydroxide particles according to claim 1.
Med magnesiumhydroksyd skal det forstås magnesiumhydroksyder av naturlig eller syntetisk opprinnelse. Naturlige magnesiumhydroksyder kan være slike som utvinnes av sjøvann, hhv. av Mg(OH)2-holdige mineraler, som f.eks. brucitt. Magnesium hydroxide is to be understood as magnesium hydroxides of natural or synthetic origin. Natural magnesium hydroxides can be those extracted from seawater, or of Mg(OH)2-containing minerals, such as brucite.
Syntetiske magnesiumhydroksyder kan være slike som f.eks. den type som markedsføres av Martinswerk GmbH i Bergheim med varemerket Magnifin®. Likeledes skal det under begrepet magnesiumhydroksyd forstås magnesiumhydroksyd-karbonater som f.eks. markedsføres av firma Microfine Minerals under varemerket Ultracarb®. Synthetic magnesium hydroxides can be such as e.g. the type marketed by Martinswerk GmbH in Bergheim under the trade mark Magnifin®. Likewise, the term magnesium hydroxide shall be understood as magnesium hydroxide carbonates such as e.g. marketed by the company Microfine Minerals under the trademark Ultracarb®.
Det er hensiktsmessig å anvende magnesiumhydroksyd-partikler som har en spesifikk overflate ifølge BET som er mindre enn 20 m<2>/g og en midlere partikkelstørelse d50 som er mindre enn 2 jum. It is appropriate to use magnesium hydroxide particles which have a specific surface according to BET which is less than 20 m<2>/g and an average particle size d50 which is less than 2 µm.
Med aluminiumhydroksyd forstås aluminiumhydroksyder av naturlig eller syntetisk opprinnelse. Naturlige aluminiumhydroksyder kan være slike som utvinnes av Al (OH) 3-holdige mineraler, som f.eks. hydrargillitt eller gibbsitt. Syntetiske aluminiumhydroksyder kan være slike som f.eks. markeds-føres av Martinswerk GmbH i Bergheim med varemerket Martifin® eller Martinal®. Aluminum hydroxide means aluminum hydroxides of natural or synthetic origin. Natural aluminum hydroxides can be those extracted from Al (OH) 3-containing minerals, such as e.g. hydrargillite or gibbsite. Synthetic aluminum hydroxides can be such as e.g. marketed by Martinswerk GmbH in Bergheim under the brand name Martifin® or Martinal®.
Ifølge oppfinnelsen er magnesiumhydroksyd- eller aluminiumhydroksyd-partiklene overflatebehandlet med en flytende etylen-propylen-kopolymer (EPM) eller en etylen-propylen-terpolymer (EPDM). Disse polymerer er også kjent under samlebegrepet "flytende elastomerer". According to the invention, the magnesium hydroxide or aluminum hydroxide particles are surface treated with a liquid ethylene-propylene copolymer (EPM) or an ethylene-propylene terpolymer (EPDM). These polymers are also known under the collective term "liquid elastomers".
Hensiktsmessige termonomerer i EPDM er diener, som f.eks. dicyklopentadien eller norbornadien. Appropriate termonomers in EPDM are dienes, such as dicyclopentadiene or norbornadiene.
Det er hensiktsmessig at disse EPM- eller EPDM-polymerer oppviser et forhold mellom etylen og propylen på mellom 40 til 60 og 60 til 40, og det er hensiktsmessig at de har en midlere molekylvekt som er lavere enn 20.000, fortrinnsvis mellom 1.000 og 15.000. Det er hensiktsmessig at jodtallet som indikerer antallet av dobbelbindinger i de forskjellige EPM- eller EPDM-polymerer ligger mellom 1 og 25. Det er hensiktsmessig at de flytende EPM- eller EPDM-polymerer anvendes i en mengde på 0,1 til 20 deler, fortrinnsvis 1 til 5 deler, pr. 100 deler magnesiumhydroksyd eller aluminiumhydroksyd. Suitably these EPM or EPDM polymers have an ethylene to propylene ratio of between 40 to 60 and 60 to 40 and suitably have an average molecular weight of less than 20,000, preferably between 1,000 and 15,000. It is appropriate that the iodine number, which indicates the number of double bonds in the various EPM or EPDM polymers, is between 1 and 25. It is appropriate that the liquid EPM or EPDM polymers are used in an amount of 0.1 to 20 parts, preferably 1 to 5 parts, per 100 parts magnesium hydroxide or aluminum hydroxide.
Magnesiumhydroksyd- eller aluminiumhydroksyd-partiklene kan videre være overflatebehandlet med en trans-polyoktenamer (TOR). Som TOR-polymerer er det hensiktsmessig å anvende slike hvor transinnholdet beveger seg mellom 40 og 90%, fortrinnsvis mellom 60 og 80%, og som har et smelte-, hhv. mykningspunkt, som hensiktsmessig ligger mellom 45 og 90°C. Det er hensiktsmessig å anvende den nevnte trans-polyoktenamer i en mengde på 0,1 til 50 deler, fortrinnsvis fra 0,5 til 5 deler, pr. 100 deler magnesiumhydroksyd eller aluminiumhydroksyd. The magnesium hydroxide or aluminum hydroxide particles can further be surface-treated with a trans-polyoctenamer (TOR). As TOR polymers, it is appropriate to use those where the trans content ranges between 40 and 90%, preferably between 60 and 80%, and which have a melting, resp. softening point, which conveniently lies between 45 and 90°C. It is appropriate to use the aforementioned trans-polyoctenamer in an amount of 0.1 to 50 parts, preferably from 0.5 to 5 parts, per 100 parts magnesium hydroxide or aluminum hydroxide.
Magnesiumhydroksydet eller aluminiumhydroksydet kan dessuten overflatebehandles med en termoplastisk elastomer (TPE), som beskrevet f.eks. i "Thermoplastische Elastomere im Aufwårtstrend", 2. fagkonferanse 10-11.10.1989, Wiirzburg, prof. dr. Muller, Siiddeutsches Kunststoffzentrum. Det er hensiktsmessig å anvende mengder på 0,1 til 50 deler, fortrinnsvis fra 0,2 til 30 deler, pr. 100 deler magnesiumhydroksyd eller aluminiumhydroksyd av følgende polymerer: EVA og EVA-kopolymerer The magnesium hydroxide or aluminum hydroxide can also be surface treated with a thermoplastic elastomer (TPE), as described e.g. in "Thermoplastische Elastomere im Aufwårtstrend", 2nd professional conference 10-11.10.1989, Wiirzburg, Prof. Dr. Muller, Siiddeutsches Kunststoffzentrum. It is appropriate to use amounts of 0.1 to 50 parts, preferably from 0.2 to 30 parts, per 100 parts magnesium hydroxide or aluminum hydroxide of the following polymers: EVA and EVA copolymers
Blokk-kopolymerer av harde og myke segmenter, som styrenelastomerer, som f.eks. SBS, SIS, SEBS termoplastiske PUR-elastomerer (TPU) Block copolymers of hard and soft segments, such as styrene elastomers, such as SBS, SIS, SEBS thermoplastic PUR elastomers (TPU)
eter-ester-blokk-kopolymerer (EEBC) ether-ester block copolymers (EEBC)
- polyeter/polyamid-blokk-kopolymerer (PEBA) termoplastiske silikonkautsjuktyper (TPQ) - polyether/polyamide block copolymers (PEBA) thermoplastic silicone rubber types (TPQ)
eller legeringer (polymerblandinger), som or alloys (polymer mixtures), which
termoplastiske polyolefiner, som oftest med polyproylen (PP) som polyolefin og en etylen-propylen-kopolymer (EPM), eller -terpolymer (EPDM) som "mykt" segment. Alternativt til polypropylen som "hard"-segment kan de amorfe til delkrystallinske termoplaster, så som thermoplastic polyolefins, most often with polypropylene (PP) as polyolefin and an ethylene-propylene copolymer (EPM), or -terpolymer (EPDM) as "soft" segment. As an alternative to polypropylene as a "hard" segment, they can be amorphous to semi-crystalline thermoplastics, such as
- polyamid (PA) - polyamide (PA)
polystyren (PS) polystyrene (PS)
styren/akrylnitril-kopolymerer (SAN) styrene/acrylonitrile copolymers (SAN)
anvendes. Som "myk" fase finnes bl.a. etylenvinylacetat (EVA) og kopolymerer av dette. are used. As a "soft" phase there are e.g. ethylene vinyl acetate (EVA) and copolymers thereof.
Foretrukket fra gruppen av termoplastiske polymerer anvendes silikonkautsjuktyper, spesielt slike som f.eks. er beskrevet i DE-OS 2 748 924, eller EVA-polymerer med et VA-innhold mellom 15 og 70%. Silicone rubber types are preferably used from the group of thermoplastic polymers, especially such as e.g. is described in DE-OS 2 748 924, or EVA polymers with a VA content between 15 and 70%.
I en foretrukket utførelsesform kan det i tillegg anvendes koplingsmidler, såkalte "coupling agents". Denne klasse av forbindelser oppviser funksjonelle grupper som sikrer at matriksen som består av (basis-)polymeren og aggregatene av magnesiumhydroksyd- eller aluminiumhydroksyd-partiklene har en best mulig kontakt med hverandre på inter-fasen, og om mulig er kovalent bundet til hverandre. In a preferred embodiment, coupling agents, so-called "coupling agents", can also be used. This class of compounds exhibits functional groups that ensure that the matrix consisting of the (base) polymer and the aggregates of the magnesium hydroxide or aluminum hydroxide particles have the best possible contact with each other at the inter-phase, and if possible are covalently bound to each other.
Egnede forbindelser for en bindingsdannelse til hydrok-sylske overflater er organosilaner, organotitanater, organo-zirko-(alumi)nater eller organoaluminater. Som organosilaner er det hensiktsmessig å anvende slike som f.eks. er beskrevet i DE-PS 2 743 682 eller som det fremgår av firmaprospektet fra Huls AG, Mari, "Anwendung von organofunktionellen Silanen, Dynasilan®, Okt. 1989". Det anvendes fortrinnsvis vinylsilaner, som f.eks. vinyltrietoksysilan eller vinyltri-metoksysilan, aminosilaner, som f.eks. aminopropyltrietoksy-silan eller metakrylsilaner, som f.eks. (metakryloyloksy-propyl)-trimetoksysilan. Som organotitanater, organo-zirko-(alumi-)nater eller organoaluminiater er det hensiktsmessig å anvende slike som er beskrevet i firmaskrivelsen "Ken-react reference manual", Bulletin KR-1084-2 fra Kenrich Petrochemicals Inc. Suitable compounds for a bond formation to hydroxyl surfaces are organosilanes, organotitanates, organo-zirco-(alumina)nates or organoaluminates. As organosilanes, it is appropriate to use such as e.g. is described in DE-PS 2 743 682 or as appears from the company prospectus from Huls AG, Mari, "Anwendung von organofunktionalen Silanen, Dynasilan®, Oct. 1989". Vinyl silanes are preferably used, such as e.g. vinyltriethoxysilane or vinyltrimethoxysilane, aminosilanes, such as e.g. aminopropyltriethoxysilane or methacrylsilanes, such as e.g. (methacryloyloxy-propyl)-trimethoxysilane. As organotitanates, organo-zirco-(aluminates) or organoaluminates, it is appropriate to use those described in the company letter "Ken-react reference manual", Bulletin KR-1084-2 from Kenrich Petrochemicals Inc.
Det er hensiktsmessig å anvende de nevnte koplingsmidler i mengder mellom 0,01 og 10 deler, fortrinnsvis mellom 0,05 og 5 deler, pr. 100 deler magnesiumhydroksyd eller aluminiumhydroksyd . It is appropriate to use the aforementioned coupling agents in amounts between 0.01 and 10 parts, preferably between 0.05 and 5 parts, per 100 parts magnesium hydroxide or aluminum hydroxide.
I en ytterligere foretrukket utførelsesform kan det i tillegg tilsettes tverrbindemidler, "interpenetrating network"-midler (IPN-midler), som bevirker en gjensidig gjennomtregning av to termodynamisk ikke-forenlige (ikke-blandbare) polyestersystemer, idet det på denne måte tillates en målrettet styring av egenskapsprofilen for forbindelsene som er forsynt med magne siximhy dr oksyd- eller aluminiumhydroksyd-partiklene. For dannelse av det interpenetrerende nettverk har slike polysiloksansystemer, hhv. polysiloksan-kopolymersystemer, fremtrådt som fordelaktige, spesielt slike som f.eks. er beskrevet i DE-OS 2 748 924. Eksempelvis anvendes polysiloksan/polystyren-kopolymerer, polysiloksan/- polykarbonat-kopolymerer, polysiloksan/polyester-kopolymerer, polysilokosan/polyamid-kopolymerer, polysiloksan/polyamid-imid-kopolymerer, polysiloksan/polyimid-kopolymerer og/eller polysiloksan/polysulfon-kopolymerer. In a further preferred embodiment, cross-linking agents, "interpenetrating network" agents (IPN agents), can also be added, which cause a mutual penetration of two thermodynamically incompatible (immiscible) polyester systems, allowing in this way a targeted controlling the property profile of the compounds provided with the magne siximhy dr oxide or aluminum hydroxide particles. For the formation of the interpenetrating network, such polysiloxane systems, or polysiloxane copolymer systems, appeared to be advantageous, especially such as e.g. is described in DE-OS 2 748 924. For example, polysiloxane/polystyrene copolymers, polysiloxane/polycarbonate copolymers, polysiloxane/polyester copolymers, polysiloxane/polyamide copolymers, polysiloxane/polyamide-imide copolymers, polysiloxane/polyimide copolymers are used and/or polysiloxane/polysulfone copolymers.
Polysiloksankomponten kan inneholde reaktive funksjonelle grupper, som f.eks. hydroksysilyl-, vinyl-, allyl-, aryl- eller metakryl-grupper. The polysiloxane component may contain reactive functional groups, such as e.g. hydroxysilyl, vinyl, allyl, aryl or methacryl groups.
Det beskrevne system inneholder i tillegg eventuelt tverrbindere av silantype med funksjonelle grupper som er i stand til å reagere med polysiloksan-komponentens silanol-funksj on. The described system also contains possibly cross-linkers of the silane type with functional groups which are capable of reacting with the silanol function of the polysiloxane component.
Det er hensiktsmessig å katalysere denne tverrbindings-reaksjon ved hjelp av egnede katalysatorer, f.eks. karboksy-later av elementene Sn, Zn, Fe, Ti, Zr eller også ved hjelp av edelmetallkatalysatorer. It is appropriate to catalyze this cross-linking reaction by means of suitable catalysts, e.g. carboxylates of the elements Sn, Zn, Fe, Ti, Zr or also with the help of noble metal catalysts.
Det er hensiktsmessig å anvende IPN-midlene i mengder på 0,1 til 20 deler pr. 100 deler fyllstoff. It is appropriate to use the IPN agents in amounts of 0.1 to 20 parts per 100 parts filler.
Eventuelt kan det tilsettes ytterligere bearbeidings-hjelpemidler, så som fettsyrer og egnede derivater av fettsyrer, eller også stabilisatorer. Optionally, further processing aids can be added, such as fatty acids and suitable derivatives of fatty acids, or also stabilizers.
For overflatemodifisering forsynes magnesiumhydroksyd-eller aluminiumhydroksyd-partiklene med de nevnte koreagenser på hensiktsmessig måte i en egnet blander, fortrinnsvis i en blander som muliggjør høye skjærkrefter. Tilsetningen kan finne sted i den valgte rekkefølge med bestemte tidsinter-valler ved forskjellige temperaturer, og med prosessparametre som er tilpasset koreagensene. Det er likeledes mulig å til-føre blanderen en forblanding av koreagensene sammen med magnesiumhydroksyd- eller aluminiumhydroksyd-partiklene. For surface modification, the magnesium hydroxide or aluminum hydroxide particles are supplied with the aforementioned core reagents in an appropriate manner in a suitable mixer, preferably in a mixer which enables high shear forces. The addition can take place in the selected order with specific time intervals at different temperatures, and with process parameters that are adapted to the core agents. It is also possible to supply the mixer with a premix of the core agents together with the magnesium hydroxide or aluminum hydroxide particles.
Det kan også være en fordel først å fremstille et additiv-konsentrat, en såkalt masterbatch, idet bare en del-mengde av fyllstoffet blandes med de koreagenser som skal anvendes ifølge den nevnte fremgangsmåte i en blander med høye skjærkrefter. Denne såkalte masterbatch kan deretter bearbeides på enkelt vis med et teknisk mindre komplisert blandeapparat, f.eks. hos kunden fortynnes med den passende mengde ytterligere fyllstoff og bearbeides til det overflatemodifiserte fyllstoff som er klart for anvendelse. It can also be advantageous to first prepare an additive concentrate, a so-called masterbatch, with only a partial amount of the filler being mixed with the co-reagents to be used according to the aforementioned method in a mixer with high shear forces. This so-called masterbatch can then be processed easily with a technically less complicated mixing device, e.g. at the customer's place, it is diluted with the appropriate amount of additional filler and processed into the surface-modified filler that is ready for use.
Det på denne måte modifiserte magnesiumhydroksyd eller aluminiumhydroksyd kan deretter bearbeides med den ønskede termoplastiske polyolefin ifølge vanlige fremgangsmåter til en compound. Som compounderingsapparater kommer vanlige blandingsapparater som kan fåes i handelen på tale, som f.eks. én- eller dobbeltskrueelter eller ko-elter. The magnesium hydroxide or aluminum hydroxide modified in this way can then be processed with the desired thermoplastic polyolefin according to usual methods into a compound. Compounding devices are common commercially available mixing devices, such as e.g. single or double screw kneader or co-kneader.
De ifølge oppfinnelsen overflatebehandlede magnesiumhydroksyd- eller aluminiumhydroksyd-partikler er egnet for flammehemmende behandling av termoplastiske polyolefiner, som f.eks. polyetylen og polyetylenkopolymerer, polypropylen eller også EVA og EVA's kopolymerer. The surface-treated magnesium hydroxide or aluminum hydroxide particles according to the invention are suitable for flame retardant treatment of thermoplastic polyolefins, such as e.g. polyethylene and polyethylene copolymers, polypropylene or also EVA and EVA's copolymers.
Vanligvis anvendes det overflatebehandlede aluminiumhydroksyd i termoplastiske polyolefiner som er bearbeidbare inntil ca. 180°C. Egnede representanter for slike termoplastiske olefiner er f.eks. EVA og EVA's kopolymerer eller polyetylen og polyetylens kopolymerer. Det overflatebehandlede magnesiumhydroksyd blir derimot vanligvis anvendt i høytemperaturområdet, dvs. i termoplastiske polymerer som er bearbeidbare fra 180 til over 300"C, fortrinnsvis i polypropylen. Eventult kan også blandinger av overflatebehandlet magnesiumhydroksyd og overflatebehandlet aluminiumhydroksyd anvendes for å gjøre termoplastiske polyolefiner flammemot-standsdyktige. Generally, the surface-treated aluminum hydroxide is used in thermoplastic polyolefins which can be processed up to approx. 180°C. Suitable representatives for such thermoplastic olefins are e.g. EVA and EVA's copolymers or polyethylene and polyethylene's copolymers. The surface-treated magnesium hydroxide, on the other hand, is usually used in the high-temperature range, i.e. in thermoplastic polymers that can be processed from 180 to over 300°C, preferably in polypropylene. Optionally, mixtures of surface-treated magnesium hydroxide and surface-treated aluminum hydroxide can also be used to make thermoplastic polyolefins flame resistant.
I forhold til de ubehandlede magnesiumhydroksyd- eller aluminiumhydroksyd-partikler oppviser de en inntil 50% høyere romvekt. Dessuten er de behandlede magnesiumhydroksyd- eller aluminiumhydroksyd-partikler frittflytende, slik at de lett lar seg dosere og er støvfri. In relation to the untreated magnesium hydroxide or aluminum hydroxide particles, they have a density up to 50% higher. In addition, the treated magnesium hydroxide or aluminum hydroxide particles are free-flowing, so that they can be easily dosed and are dust-free.
Innholdet av overflatebehandlet materiale i den an-gjeldende polymermatriks beveger seg vanligvis mellom 50 og 70%, fortrinnsvis tenderer det mot de lavere prosentinnhold innenfor den nevnte båndbredde, for å minimere påvirkningen av compoundens mekaniske egenskapsbilde. The content of surface-treated material in the relevant polymer matrix usually ranges between 50 and 70%, preferably tending towards the lower percentages within the aforementioned bandwidth, in order to minimize the influence on the compound's mechanical properties.
Compoundene som inneholder magnesiumhydroksyd- eller aluminiumhydroksyd-partiklene kan i tillegg inneholde fiber-formede forsterkningsstoffer. Til fiberstoffene hører eksempelvis glassfibre, steinfibre, metallfibre, poly-krystallinske keramiske fibre, inkludert énkrystallene, de såkalte "whiskers", samt alle fibre som stammer fra syntetiske polymerer, som f.eks. aramid-, karbon-, polyamid-, polyakryl-, polyester- og polyetylenfibre. The compounds containing the magnesium hydroxide or aluminum hydroxide particles may also contain fibre-shaped reinforcing substances. The fibrous materials include, for example, glass fibres, stone fibres, metal fibres, poly-crystalline ceramic fibres, including the single crystals, the so-called "whiskers", as well as all fibers originating from synthetic polymers, such as e.g. aramid, carbon, polyamide, polyacrylic, polyester and polyethylene fibres.
Dersom det er ønsket, kan compoundene tilsettes egnede pigmenter og/eller farvestoffer. If desired, suitable pigments and/or dyes can be added to the compounds.
Det ble oppnådd en fremragende slagseighet ved avveid egenskapsprofil for polymermatriksen når magnesiumhydroksyd-eller aluminiumhydroksyd-partiklene ble overflatebehandlet med en flytende EPM- eller EPDM-polymer og i tillegg med en i det foregående nevnte trans-polyoktenamer (TOR). An outstanding impact resistance was achieved by weighted property profile for the polymer matrix when the magnesium hydroxide or aluminum hydroxide particles were surface treated with a liquid EPM or EPDM polymer and additionally with a previously mentioned trans-polyoctenamer (TOR).
Det oppnås en svært god strekkfasthet ved avveid god egenskapsprofil for polymermatriksen når magnesiumhydroksyd-eller aluminiumhydroksyd-partiklene er overflatebehandlet med en flytende EPM- eller EPDM-polymer, samt i tillegg med en vinylsilan som koplingsmiddel. A very good tensile strength is achieved with a balanced good property profile for the polymer matrix when the magnesium hydroxide or aluminum hydroxide particles are surface treated with a liquid EPM or EPDM polymer, and additionally with a vinyl silane as a coupling agent.
Overraskende avveide gode egenskapsprofiler for polymermatriksen ble oppnådd ved hjelp av følgende kombinasjon: magnesiumhydroksyd- eller aluminiumhydroksyd-partikler/- EPM- eller EPDM-polymer/TOR/vinylsilan som koplingsmidler, Surprisingly balanced good property profiles for the polymer matrix were obtained using the following combination: magnesium hydroxide or aluminum hydroxide particles/- EPM or EPDM polymer/TOR/vinyl silane as coupling agents,
magnesiumhydroksyd- eller aluminiumhydroksyd-partikler/- magnesium hydroxide or aluminum hydroxide particles/-
TOR/IPN-danner, TOR/IPN generator,
magnesiumhydroksyd- eller aluminiumhydroksyd-partikler/- magnesium hydroxide or aluminum hydroxide particles/-
TOR/termoplastisk elastomer. TOR/thermoplastic elastomer.
Sammenligningseksempel 1 Comparative example 1
10 kg magnesiumhydroksyd Kisuma 5A fra Kyowa Chemical Ind., og som er overflatemodifisert ifølge DE-PS 2 659 933, ble bearbeidet til en compound med polypropylen-homopolymer med en midlere molekylvekt på 4,4 "105 (Vestolen PP 8400 fra Huls) på et énskrueapparat, slik at compounden inneholdt 35% polypropylen og 65% modifisert magnesiumhydroksyd. 10 kg of magnesium hydroxide Kisuma 5A from Kyowa Chemical Ind., which is surface modified according to DE-PS 2 659 933, was processed into a compound with polypropylene homopolymer with an average molecular weight of 4.4 "105 (Vestolen PP 8400 from Huls) on a single-screw device, so that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Sammenligningseksempel 2 Comparative example 2
I en intensivblander (fluid-/kjøleblander-kombinasjon) ble 10 kg magnesiumhydroksyd Magnifin H 10 (fra Martinswerk GmbH) med en midlere kornstørrelse på 1 ym. og en midlere spesifikk overflate ifølge BET på 10 m<2>/g fluidisert ved en temperatur på 50°C. I løpet av 60 sekunder ble 0,1 kg av en flytende etylen-propylen-terpolymer (EPDM) med dicyklopentadien som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) tilsatt i en konstant strøm til det agiterte fyllstoff. Etter 5 minutter ble sluttemperaturen på 80 til 100°C oppnådd, og det modifiserte magnesiumhydroksyd ble ført ut i kjøleblanderen. Det oppnådde produkt ble bearbeidet til en compound med en polypropylen-homopolymer med en midlere molekylvekt på 4,4 "105 (Vestolen PP 8400 fra Hiils) på et énskrueapparat på en slik måte at compounden inneholdt 3 5% polypropylen og 65% modifisert magnesiumhydroksyd. In an intensive mixer (fluid/refrigerator mixer combination), 10 kg of magnesium hydroxide Magnifin H 10 (from Martinswerk GmbH) with an average grain size of 1 µm. and an average specific surface according to BET of 10 m<2>/g fluidized at a temperature of 50°C. During 60 seconds, 0.1 kg of a liquid ethylene-propylene terpolymer (EPDM) with dicyclopentadiene as thermonomer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) was added in a constant stream to the agitated filler. After 5 minutes, the final temperature of 80 to 100°C was reached and the modified magnesium hydroxide was discharged into the cooling mixer. The obtained product was processed into a compound with a polypropylene homopolymer with an average molecular weight of 4.4 "105 (Vestolen PP 8400 from Hiils) on a single-screw apparatus in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Eksempel l Example l
15 kg magnesiumhydroksyd Magnifin H 10 (fra Martinswerk GmbH) med en midlere kornstørrelse på 1 /Ltm og med en midlere spesifikk overflate ifølge BET på 10 m<2>/g, og som var behandlet med 0,15 kg vinylsilan (A 172, Union Carbide), ble fluidisert i intensivblanderen (fluid-/kjøleblander-kombinasjon), til det var oppnådd en temperatur på ca. 50°C. I løpet av 90 sekunder ble en blanding av 0,69 kg av en flytende etylen/propylen-kopolymer (EPM) med en midlere molekylvekt på 7200 (Trilene CP 80, Uniroyal) og 0,3 kg av en styren/- butadienelastomer (Kraton G, Shell) som termoplastisk elastomer tilsatt med konstant hastighet til det agiterte fyllstoff. Da satstemperaturen hadde nådd 100°C, ble produktet ført ut i kjøleblanderen. Det på denne måte modifiserte fyllstoff var karakterisert ved en 50% høyere romvekt, støvfrihet og god doserbarhet. Det oppnådde produkt ble bearbeidet med en polypropylen-homopolymer med en midlere molekylvekt på 4,4 "IO5 (Vestolen PP 8400 fra Hiils) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% polypropylen og 65% modifisert magnesiumhydroksyd. 15 kg of magnesium hydroxide Magnifin H 10 (from Martinswerk GmbH) with an average grain size of 1 /Ltm and with an average specific surface according to BET of 10 m<2>/g, and which was treated with 0.15 kg of vinyl silane (A 172, Union Carbide), was fluidized in the intensive mixer (fluid/refrigerator mixer combination), until a temperature of approx. 50°C. During 90 seconds, a mixture of 0.69 kg of a liquid ethylene/propylene copolymer (EPM) with an average molecular weight of 7200 (Trilene CP 80, Uniroyal) and 0.3 kg of a styrene/butadiene elastomer (Kraton G, Shell) as a thermoplastic elastomer added at a constant rate to the agitated filler. When the batch temperature had reached 100°C, the product was fed into the cooling mixer. The filler modified in this way was characterized by a 50% higher bulk density, freedom from dust and good dosing. The obtained product was processed with a polypropylene homopolymer with an average molecular weight of 4.4 "IO5 (Vestolen PP 8400 from Hiils) on a single-screw apparatus into a compound in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Eksempel 2 Example 2
I intensivblanderen (fluid-/kjøleblander-kombinasjon) ble det anbrakt 15 kg magnesiumhydroksyd Magnifin H 10 (fra Martinswerk GmbH) med en midlere kornstørrelse på 1 /xm og en midlere spesifikk overflate ifølge BET på 10 m<2>/g, og 1,4 kg av et ifølge sammenligningseksempel 2 fremstilt overflatebehandlet magnesiumhydroksyd i form av en konsentratblanding med 55% Mg(OH)2-innhold ble tilført den stående blander. Etter at satsen var fluidisert i 5 minutter, var blandetemperaturen ca. 80 til 100"C. Produktet ble ført ut i en kjøleblander og så straks tilsatt 0,15 kg vinyltrietoksysilan som koplingsmiddel. Under avkjølingsfasen til 35"C ble vinyltrietoksysilanet innarbeidet på homogent vis. Det på denne måte modifiserte fyllstoff utmerket seg ved en 30% høyere romvekt, høy fluididet og følgelig svært god doseringsevne og støvfrihet. Det oppnådde produkt ble bearbeidet med en polypropylen-homopolymer med en midlere molekylvekt på 4,4 "IO5 (Vestolen PP 8400 fra Hiils) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% polypropylen og 65% modifisert magnesiumhydroksyd. 15 kg of magnesium hydroxide Magnifin H 10 (from Martinswerk GmbH) with an average grain size of 1 /xm and an average specific surface according to BET of 10 m<2>/g was placed in the intensive mixer (fluid/refrigerator mixer combination), and 1 .4 kg of a surface-treated magnesium hydroxide produced according to comparative example 2 in the form of a concentrate mixture with 55% Mg(OH)2 content was added to the standing mixer. After the batch had been fluidized for 5 minutes, the mixing temperature was approx. 80 to 100°C. The product was fed into a cooling mixer and then immediately added 0.15 kg of vinyltriethoxysilane as a coupling agent. During the cooling phase to 35°C, the vinyltriethoxysilane was incorporated homogeneously. The filler modified in this way was distinguished by a 30% higher bulk density, high fluidity and consequently very good dosing ability and freedom from dust. The obtained product was processed with a polypropylene homopolymer with an average molecular weight of 4.4 "IO5 (Vestolen PP 8400 from Hiils) on a single-screw apparatus into a compound in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Eksempel 3 Example 3
I intensivblanderen (fluid-/kjøleblander-kombinasjon) ble 10 kg magnesiumhydroksyd Magnifin H 10 (fra Martinswerk GmbH) med en midlere kornstørrelse på 1 //m og en midlere spesifikk overflate ifølge BET på 10 m<2>/g, blandet med 200 g (2,0 vekt%) vinylsilan (A 172, Union Carbide) og 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien (DCPD) som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) i tilsammen 10 minutter med en sluttemperatur på 50 til 70°C. Det oppnådde produkt ble bearbeidet med en polypropylen-homopolymer med en midlere molekylvekt på 4,4 "105 (Vestolen PP 8400 fra Hiils) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% polypropylen og 65% modifisert magnesiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination), 10 kg of magnesium hydroxide Magnifin H 10 (from Martinswerk GmbH) with an average grain size of 1 //m and an average specific surface according to BET of 10 m<2>/g, was mixed with 200 g (2.0% by weight) vinyl silane (A 172, Union Carbide) and 300 g (3.0% by weight) liquid EPDM with dicyclopentadiene (DCPD) as thermonomizer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) in total 10 minutes with a final temperature of 50 to 70°C. The obtained product was processed with a polypropylene homopolymer with an average molecular weight of 4.4 "105 (Vestolen PP 8400 from Hiils) on a single-screw apparatus into a compound in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Eksempel 4Example 4
I intensivblanderen (fluid-/kjøleblander-kombinasjon) ble 10 kg magnesiumhydroksyd Magnifin H 10 (fra Martinswerk GmbH) med en midlere kornstørrelse på 1 ^m og en midlere spesifikk overflate ifølge BET på 10 m<2>/g, blandet med 460 g (4,6 vekt%) flytende EPDM med dicyklopentadien som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) og med 310 g (3,1 vekt%) trans-polyoktenamer (TOR) med 80% trans-innhold (Vestenamer 8012 fra Hiils) og et mykningsområde 55 og 70°C i tilsammen 10 minutter med en sluttemperatur på 50 til 70°C. Det oppnådde produkt ble bearbeidet med en polypropylen-homopolymer med en midlere molekylvekt på 4,4"10<5 >(Vestolen P 8400 fra Hiils) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% polypropylen og 65% modifisert magnesiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination) 10 kg of magnesium hydroxide Magnifin H 10 (from Martinswerk GmbH) with an average grain size of 1 µm and an average specific surface according to BET of 10 m<2>/g was mixed with 460 g (4.6% by weight) liquid EPDM with dicyclopentadiene as thermonomer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) and with 310 g (3.1% by weight) trans-polyoctenamer (TOR) with 80% trans content ( Vestenamer 8012 from Hiils) and a softening range of 55 and 70°C for a total of 10 minutes with a final temperature of 50 to 70°C. The product obtained was processed with a polypropylene homopolymer with an average molecular weight of 4.4"10<5> (Vestolen P 8400 from Hiils) on a single-screw apparatus into a compound in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Eksempel 5 Example 5
I intensivblanderen (fluid-/kjøleblander-kombinasjon) ble 10 kg magnesiumhydroksyd Magnifin H 10 (fra Martinswerk GmbH) med en midlere kornstørrelse på 1 /nm og en midlere spesifikk overflate ifølge BET på 10 m<2>/g, blandet med 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal), og med 200 g (2,0 vekt%) etylenvinylacetat (Escorene Ultra UL 04028), med 100 g (1,0 vekt%) zirkoniumlaurat med 200 g (2,0 vekt%) tverrbundet polyetylen (Vistaflex, Exxon) som termoplastisk elastomer i 10 minutter med en sluttemperatur på 50 til 70°C. Det oppnådde produkt ble bearbeidet med en polypropylen-homopolymer med en midlere molekylvekt på 4,4"10<5 >(Vestolen PP 8400 fra Hiils) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% polypropylen og 65% modifisert magnesiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination), 10 kg of magnesium hydroxide Magnifin H 10 (from Martinswerk GmbH) with an average grain size of 1 /nm and an average specific surface according to BET of 10 m<2>/g, was mixed with 300 g (3.0 wt%) liquid EPDM with dicyclopentadiene as thermonomizer and with an average molecular weight of 7000 (Trilene 65, Uniroyal), and with 200 g (2.0 wt%) ethylene vinyl acetate (Escorene Ultra UL 04028), with 100 g ( 1.0 wt%) zirconium laurate with 200 g (2.0 wt%) cross-linked polyethylene (Vistaflex, Exxon) as thermoplastic elastomer for 10 minutes with a final temperature of 50 to 70°C. The obtained product was processed with a polypropylene homopolymer with an average molecular weight of 4.4"10<5> (Vestolen PP 8400 from Hiils) on a single-screw apparatus into a compound in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Eksempel 6 Example 6
I intensivblanderen (fluid-/kjøleblander-kombinasjon) ble 10 kg magnesiumhydroksyd Magnifin H 10 (fra Martinswerk GmbH) med en midlere kornstørrelse på 1 ^m og en midlere spesifikk overflate ifølge BET på 10 m<2>/g, blandet med 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal), med 200 g (2,0 vekt%) av et etylenvinylacetat (Escorene Ultra UL 04028, Exxon) som termoplastisk elastomer og med 100 g In the intensive mixer (fluid/refrigerator mixer combination) 10 kg of magnesium hydroxide Magnifin H 10 (from Martinswerk GmbH) with an average grain size of 1 µm and an average specific surface according to BET of 10 m<2>/g was mixed with 300 g (3.0 wt%) liquid EPDM with dicyclopentadiene as thermonomizer and with an average molecular weight of 7000 (Trilene 65, Uniroyal), with 200 g (2.0 wt%) of an ethylene vinyl acetate (Escorene Ultra UL 04028, Exxon) as thermoplastic elastomer and with 100 g
(1,0 vekt%) laurinsyre i tilsammen 10 minutter med en sluttemperatur på 50 til 70°C. Det oppnådde produkt ble (1.0 wt%) lauric acid for a total of 10 minutes with a final temperature of 50 to 70°C. The product obtained was
bearbeidet med en polypropylen-homopolymer med en midlere molekylvekt på 4,4 "IO5 (Vestolen PP 8400 fra Hiils) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% polypropylen og 65% modifisert magnesiumhydroksyd . processed with a polypropylene homopolymer with an average molecular weight of 4.4 "IO5 (Vestolen PP 8400 from Hiils) on a single-screw apparatus into a compound in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Eksempel 7 Example 7
I intensivblanderen (fluid-/kjøleblander-kombinasjon) ble 10 kg magnesiumhydroksyd Magnifin H 10 (fra Martinswerk GmbH) med en midlere kornstørrelse på 1 ^ ra. og en midlere spesifikk overflate ifølge BET på 10 m<2>/g, blandet med 50 g (0,5 vekt%) av et kvaternært zirkonat (NZ 38 J, Kenrich) og 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien (DCPD) som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) og 200 g (2,0 vekt%) PEBA (Pebax Atochem) i tilsammen 10 minutter med en sluttemperatur på 50 til 70°C. Det oppnådde produkt ble bearbeidet med en polypropylen-homopolymer med en midlere molekylvekt på 4,4 "10<5> (Vestolen PP 8400 fra Hiils) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 3 5% polypropylen og 65% modifisert magnesiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination) 10 kg of magnesium hydroxide Magnifin H 10 (from Martinswerk GmbH) with an average grain size of 1 ra. and an average specific surface according to BET of 10 m<2>/g, mixed with 50 g (0.5 wt%) of a quaternary zirconate (NZ 38 J, Kenrich) and 300 g (3.0 wt%) of liquid EPDM with dicyclopentadiene (DCPD) as thermonomer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) and 200 g (2.0% by weight) PEBA (Pebax Atochem) for a total of 10 minutes with a final temperature of 50 to 70°C. The product obtained was processed with a polypropylene homopolymer with an average molecular weight of 4.4 "10<5> (Vestolen PP 8400 from Hiils) on a single-screw apparatus into a compound in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Eksempel 8 Example 8
I intensivblanderen (fluid-/kjøleblander-kombinasjon) ble 10 kg magnesiumhydroksyd Magnifin H 10 (fra Martinswerk GmbH) med en midlere kornstørrelse på 1 jum og en midlere spesifikk overflate ifølge BET på 10 m<2>/g, blandet med 100 g (1,0 vekt%) av et organopolysiloksan (SFR 100, General Electric Silicones) og 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien (DCPD) som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) og 200 g (2,0 vekt%) Aminosilan (A 1100, Union Carbide) i tilsammen 10 minutter med en sluttemperatur på 50 til 70"C. Det oppnådde produkt ble bearbeidet med en polypropylen-homopolymer med en midlere molekylvekt på 4,4 "IO5 (Vestolen PP 8400 fra Hiils) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% polypropylen og 65% modifisert magnesiumhydroksyd. In the intensive mixer (fluid/refrigerated mixer combination), 10 kg of magnesium hydroxide Magnifin H 10 (from Martinswerk GmbH) with an average grain size of 1 µm and an average specific surface according to BET of 10 m<2>/g was mixed with 100 g ( 1.0 wt%) of an organopolysiloxane (SFR 100, General Electric Silicones) and 300 g (3.0 wt%) of liquid EPDM with dicyclopentadiene (DCPD) as thermonomizer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) and 200 g (2.0% by weight) Aminosilane (A 1100, Union Carbide) for a total of 10 minutes with a final temperature of 50 to 70"C. The product obtained was processed with a polypropylene homopolymer with an average molecular weight of 4.4" IO5 (Vestolen PP 8400 from Hiils) on a single screw device to a compound in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Eksempel 9 Example 9
I intensivblanderen (fluid-/kjøleblander-kombinasjon) ble 10 kg magnesiumhydroksyd-karbonat Ultracarb® (fra Microfine Minerals) med en midlere spesifikk overflate ifølge BET på 15 m<2>/g, blandet med 200 g (2,0 vekt%) vinylsilan (A 172, Union Carbide) og 300 g (3,0 vekt%) flytende EPM med en midlere molekylvekt på 7200 (Trilene CP 80, Uniroyal) i tilsammen 10 minutter med en sluttemperatur på 50 til 70"C. Det oppnådde produkt ble bearbeidet med en polypropylen-homopolymer med en midlere molekylvekt på 4,4 "105 (Vestolen PP 8400 fra Hiils) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% polypropylen og 65% modifisert magnesiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination) 10 kg of magnesium hydroxide carbonate Ultracarb® (from Microfine Minerals) with an average specific surface according to BET of 15 m<2>/g, was mixed with 200 g (2.0 wt%) vinyl silane (A 172, Union Carbide) and 300 g (3.0 wt%) of liquid EPM with an average molecular weight of 7200 (Trilene CP 80, Uniroyal) for a total of 10 minutes with a final temperature of 50 to 70°C. The product obtained was processed with a polypropylene homopolymer with an average molecular weight of 4.4 "105 (Vestolen PP 8400 from Hiils) on a single-screw apparatus into a compound in such a way that the compound contained 35% polypropylene and 65% modified magnesium hydroxide.
Sammenligningseksempel Comparative example
I intensivblanderen (fluid-/kjøleblander-kombinasjon) ble 10 kg aluminiumhydroksyd Marital OL 107 (fra Martinswerk GmbH) med en midlere kornstørrelse på 0,9 - 1,3 /im og en midlere spesifikk overflate ifølge BET på 6 - 8 m<2>/g fluidisert ved en temperatur på 50°C. I løpet av 60 sekunder ble 0,1 kg av en flytende etylen-propylen-terpolymer (EPDM) med dicyklopentadien som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) tilsatt med konstant hastighet til det agiterte fyllstoff. Etter 5 minutter var slutt-temperaturen på 80 til 100°C oppnådd, og det modifiserte aluminiumhydroksyd ble tatt ut av kjøleblanderen. Det oppnådde produkt ble bearbeidet med en EVA-polymer (Escorene Ultra UL 0202 0, Exxon) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% EVA-polymer og 65% modifisert aluminiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination) 10 kg of aluminum hydroxide Marital OL 107 (from Martinswerk GmbH) with an average grain size of 0.9 - 1.3 µm and an average specific surface according to BET of 6 - 8 m<2 >/g fluidized at a temperature of 50°C. During 60 seconds, 0.1 kg of a liquid ethylene-propylene terpolymer (EPDM) with dicyclopentadiene as thermonomer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) was added at a constant rate to the agitated filler. After 5 minutes, the final temperature of 80 to 100°C was reached and the modified aluminum hydroxide was removed from the cooling mixer. The product obtained was processed with an EVA polymer (Escorene Ultra UL 0202 0, Exxon) on a single screw apparatus into a compound in such a way that the compound contained 35% EVA polymer and 65% modified aluminum hydroxide.
Eksempel 10 Example 10
15 kg aluminiumhydroksyd Marital OL 107 (fra Martinswerk GmbH) med en midlere kornstørrelse på 0,9 - 1,3 nm og med en midlere spesifikk overflate ifølge BET på 6 - 8 m<2>/g, og som var behandlet med 0,15 kg vinylsilan (A 172, Union Carbide) ble fluidisert i intensivblanderen (fluid-/kjøleblander-kombinasjon) til det var oppnådd en temperatur på ca. 50°C. I løpet av 90 sekunder ble en blanding av 0,69 kg av en flytende etylen-propylen-kopolymer (EPM) med en midlere molekylvekt på 7200 (Trilene CP 80, Uniroyal) og 0,3 kg av en styren-butadienelastomer (Kraton G, Shell) som termoplastisk elastomer tilsatt med konstant hastighet til det agiterte fyllstoff. Da satstemperaturen hadde nådd 100°C, ble produktet ført ut i kjøleblanderen. Det på denne måte modifiserte fyllstoff var karakterisert ved en 50% høyere romvekt, støvfrihet og god doserbarhet. Det oppnådde produkt ble bearbeidet med en EVA-polymer (Escorene Ultra UL 02 020, Exxon) på et énskrueapparat til en compound på en slik måte at compounden inneholdt 35% EVA-polymer og 65% modifisert aluminiumhydroksyd. 15 kg of aluminum hydroxide Marital OL 107 (from Martinswerk GmbH) with an average grain size of 0.9 - 1.3 nm and with an average specific surface according to BET of 6 - 8 m<2>/g, and which was treated with 0, 15 kg of vinyl silane (A 172, Union Carbide) was fluidized in the intensive mixer (fluid/refrigerator mixer combination) until a temperature of approx. 50°C. During 90 seconds, a mixture of 0.69 kg of a liquid ethylene-propylene copolymer (EPM) with an average molecular weight of 7200 (Trilene CP 80, Uniroyal) and 0.3 kg of a styrene-butadiene elastomer (Kraton G , Shell) as a thermoplastic elastomer added at a constant rate to the agitated filler. When the batch temperature had reached 100°C, the product was fed into the cooling mixer. The filler modified in this way was characterized by a 50% higher bulk density, freedom from dust and good dosing. The obtained product was processed with an EVA polymer (Escorene Ultra UL 02 020, Exxon) on a single-screw apparatus into a compound in such a way that the compound contained 35% EVA polymer and 65% modified aluminum hydroxide.
Eksempel 11 Example 11
I intensivblanderen (fluid-/kjøleblanderkombinasjon) ble det anbraskt 15 kg aluminiumhydroksyd Martinal OL 107 (fra Martinswerk GmbH) med en midlere kornstørrelse på 0,9 - In the intensive mixer (fluid/refrigerator mixer combination) 15 kg of aluminum hydroxide Martinal OL 107 (from Martinswerk GmbH) with an average grain size of 0.9 -
1,3 nm og en midlere spesifikk overflate ifølge BET på 6 - 1.3 nm and an average specific surface according to BET of 6 -
8 m<2>/g, og i den stående blander ble det tilsatt 1,4 kg av et ifølge sammenligningseksempel 2 fremstilt overflatebehandlet aluminiumhydroksyd i form av en konsentratblanding med 55% Al (OH) 3-innhold. Etter at satsen var fluidisert i 5 minutter, var blandetemperaturen ca. 80 til 100°C. Produktet ble ført ut i en kjøleblander og så straks tilsatt 0,15 kg vinyltrietoksysilan som koplingsmiddel. Under avkjølingsfasen til 35"C ble vinyltrietoksysilanet innarbeidet på homogent vis. Det på denne måte modifiserte fyllstoff utmerket seg ved en 30% høyere romvekt, høy fluiditet og følgelig svært god doseringsevne og støvfrihet. Det oppnådde produkt ble bearbeidet med en EVA-polymer (Escorene Ultra UL 02020, Exxon), til en compound på et énskrueapparat, slik at compounden inneholdt 35% EVA-polymer og 65% modifisert aluminiumhydroksyd . 8 m<2>/g, and 1.4 kg of a surface-treated aluminum hydroxide prepared according to comparative example 2 was added in the form of a concentrate mixture with 55% Al (OH) 3 content. After the batch had been fluidized for 5 minutes, the mixing temperature was approx. 80 to 100°C. The product was fed into a cooling mixer and then immediately added 0.15 kg of vinyltriethoxysilane as a coupling agent. During the cooling phase to 35"C, the vinyltriethoxysilane was incorporated homogeneously. The filler modified in this way excelled with a 30% higher bulk density, high fluidity and consequently very good dosing ability and freedom from dust. The obtained product was processed with an EVA polymer (Escorene Ultra UL 02020, Exxon), to a compound on a single screw device, so that the compound contained 35% EVA polymer and 65% modified aluminum hydroxide.
Eksempel 12 Example 12
I intensivblanderen (fluid-/kjøleblanderkombinasjon) ble 10 kg aluminiumhydroksyd Martinal OL 107 (fra Martinswerk GmbH) med en midlere kornstørrelse på ca. 0,9 - 1,3 /xm og en midlere spesifikk overflate ifølge BET på 6 - 8 m<2>/g blandet med 200 g (2,0 vekt%) vinylsilan (A 172, Union Carbide) og 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien (DCPD) som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) i tilsammen 10 minutter med en sluttemperatur på 50 til 70°C. Det oppnådde produkt ble bearbeidet med en EVA-polymer (Escorene Ultra UL 02 02 0, Exxon), til en compound på et énskrueapparat, slik at compounden inneholdt 35% EVA-polymer og 65% modifisert aluminiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination), 10 kg of aluminum hydroxide Martinal OL 107 (from Martinswerk GmbH) with an average grain size of approx. 0.9 - 1.3 /xm and an average specific surface according to BET of 6 - 8 m<2>/g mixed with 200 g (2.0% by weight) vinyl silane (A 172, Union Carbide) and 300 g (3 .0 weight%) liquid EPDM with dicyclopentadiene (DCPD) as thermonomer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) for a total of 10 minutes with a final temperature of 50 to 70°C. The product obtained was processed with an EVA polymer (Escorene Ultra UL 02 02 0, Exxon) into a compound on a single-screw apparatus, so that the compound contained 35% EVA polymer and 65% modified aluminum hydroxide.
Eksempel 13 Example 13
I intensivblanderen (fluid-/kjøleblanderkombinasjon) ble 10 kg aluminiumhydroksyd Martinal OL 107 (fra Martinswerk GmbH) med en midlere kornstørrelse på ca. 0,9 - 1,3 ^m og en midlere spesifikk overflate ifølge BET på 6 - 8 m<2>/g blandet med 460 g (4,6 vekt%) flytende EPDM med dicyklopentadien som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) og med 310 g (3,1 vekt%) trans-poly-oktenamer (TOR) med 80% trans-innhold (Vestenamer 8012 fra Hiils) og et mykningsområde mellom 55 og 70°C i tilsammen 10 minutter med en sluttemperatur på 50 til 70°C. Det oppnådde produkt ble bearbeidet med en EVA-polymer (Escorene Ultra UL 02020, Exxon), til en compound på et énskrueapparat, slik at compounden inneholdt 35% EVA-polymer og 65% modifisert aluminiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination), 10 kg of aluminum hydroxide Martinal OL 107 (from Martinswerk GmbH) with an average grain size of approx. 0.9 - 1.3 ^m and an average specific surface according to BET of 6 - 8 m<2>/g mixed with 460 g (4.6% by weight) of liquid EPDM with dicyclopentadiene as thermonomer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) and with 310 g (3.1% by weight) trans-poly-octenamer (TOR) with 80% trans content (Vestenamer 8012 from Hiils) and a softening range between 55 and 70°C for a total of 10 minutes with a final temperature of 50 to 70°C. The obtained product was processed with an EVA polymer (Escorene Ultra UL 02020, Exxon) into a compound on a single-screw apparatus, so that the compound contained 35% EVA polymer and 65% modified aluminum hydroxide.
Eksempel 14 Example 14
I intensivblanderen (fluid-/kjøleblanderkombinasjon) ble 10 kg aluminiumhydroksyd Martinal OL 107 (fra Martinswerk GmbH) med en midlere kornstørrelse på ca. 0,9 - 1,3 jum og en midlere spesifikk overflate ifølge BET på 6 - 8 m<2>/g blandet med 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal), med 200 g (2,0 vekt%) etylenvinylacetat (Escorene Ultra UL 04028, Exxon), med 100 g (1,0 vekt%) zirkoniumlaurat med 200 g (2,0 vekt%) tverrbundet polyetylen (Vistaflex Exxon) som termoplastisk elastomer i 10 minutter med en sluttemperatur på 50 til 70"C. Det oppnådde produkt ble bearbeidet med en EVA-polymer (Escorene Ultra UL 02020, Exxon), til en compound på et énskrueapparat, slik at compounden inneholdt 3 5% EVA-polymer og 65% modifisert aluminiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination), 10 kg of aluminum hydroxide Martinal OL 107 (from Martinswerk GmbH) with an average grain size of approx. 0.9 - 1.3 µm and an average specific surface according to BET of 6 - 8 m<2>/g mixed with 300 g (3.0% by weight) liquid EPDM with dicyclopentadiene as thermonomizer and with an average molecular weight of 7000 Trilene 65, Uniroyal), with 200 g (2.0 wt%) ethylene vinyl acetate (Escorene Ultra UL 04028, Exxon), with 100 g (1.0 wt%) zirconium laurate with 200 g (2.0 wt%) crosslinked polyethylene ( Vistaflex Exxon) as thermoplastic elastomer for 10 minutes with a final temperature of 50 to 70"C. The obtained product was processed with an EVA polymer (Escorene Ultra UL 02020, Exxon) into a compound on a single-screw apparatus, so that the compound contained 3 5% EVA polymer and 65% modified aluminum hydroxide.
Eksempel 15 Example 15
I intensivblanderen (fluid-/kjøleblanderkombinasjon) ble 10 kg aluminiumhydroksyd Martinal OL 107 (fra Martinswerk GmbH) med en midlere kornstørrelse på ca. 0,9 - 1,3 /im og en midlere spesifikk overflate ifølge BET på 6 - 8 m<2>/g blandet med 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal), med 200 g (2,0 vekt%) etylenvinylacetat (Escorene Ultra UL 04028, Exxon) som termoplastisk elastomer og med 100 g (1,0 vekt%) laurinsyre i tilsammen 10 minutter med en slutt-temperatur på 50 til 70°C. Det oppnådde produkt ble bearbeidet med en EVA-polymer (Escorene Ultra UL 02020, Exxon), til en compound på et énskrueapparat, slik at compounden inneholdt 35% EVA-polymer og 65% modifisert aluminiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination), 10 kg of aluminum hydroxide Martinal OL 107 (from Martinswerk GmbH) with an average grain size of approx. 0.9 - 1.3 /im and an average specific surface area according to BET of 6 - 8 m<2>/g mixed with 300 g (3.0% by weight) liquid EPDM with dicyclopentadiene as thermonomer and with an average molecular weight of 7000 (Trilene 65, Uniroyal), with 200 g (2.0 wt%) ethylene vinyl acetate (Escorene Ultra UL 04028, Exxon) as thermoplastic elastomer and with 100 g (1.0 wt%) lauric acid for a total of 10 minutes with a final temperature of 50 to 70°C. The obtained product was processed with an EVA polymer (Escorene Ultra UL 02020, Exxon) into a compound on a single-screw apparatus, so that the compound contained 35% EVA polymer and 65% modified aluminum hydroxide.
Eksempel 16 Example 16
I intensivblanderen (fluid-/kjøleblanderkombinasjon) ble 10 kg aluminiumhydroksyd Martinal OL 107 (fra Martinswerk GmbH) med en midlere kornstørrelse på ca. 0,9 - 1,3 /xm og en midlere spesifikk overflate ifølge BET på 6 - 8 m<2>/g blandet med 50 g (0,5 vekt%) av et kvat. zirkonat (NZ 38 J Kenrich) og 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien (DCPD) som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) og 2 00 g (2,0 vekt%) PEBA (Pebax Atochem) i tilsammen 10 minutter med en sluttemperatur på 50 til 70"C. Det oppnådde produkt ble bearbeidet med en EVA-polymer (Escorene Ultra UL 02020, Exxon), til en compound på et énskrueapparat, slik at compounden inneholdt 35% EVA-polymer og 65% modifisert aluminiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination), 10 kg of aluminum hydroxide Martinal OL 107 (from Martinswerk GmbH) with an average grain size of approx. 0.9 - 1.3 /xm and an average specific surface according to BET of 6 - 8 m<2>/g mixed with 50 g (0.5% by weight) of a quat. zirconate (NZ 38 J Kenrich) and 300 g (3.0 wt%) of liquid EPDM with dicyclopentadiene (DCPD) as thermonomizer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) and 200 g (2.0 wt%) PEBA (Pebax Atochem) for a total of 10 minutes with a final temperature of 50 to 70"C. The obtained product was processed with an EVA polymer (Escorene Ultra UL 02020, Exxon) into a compound on a single-screw apparatus, so that the compound contained 35 % EVA polymer and 65% modified aluminum hydroxide.
Eksempel 17 Example 17
I intensivblanderen (fluid-/kjøleblanderkombinasjon) ble 10 kg aluminiumhydroksyd Martinal OL 107 (fra Martinswerk GmbH) med en midlere kornstørrelse på ca. 0,9 - 1,3 jxm og en midlere spesifikk overflate ifølge BET på 6 - 8 m<2>/g blandet med 100 g (1,0 vekt%) av et organopolysiloksan (SFR 100, General Electric Silicones) og 300 g (3,0 vekt%) flytende EPDM med dicyklopentadien (DCPD) som termonomer og med en midlere molekylvekt på 7000 (Trilene 65, Uniroyal) og 200 g (2 vekt%) aminosilan (A 1100, Union Carbide) i tilsammen 10 minutter med en sluttemperatur på 50 til 70°C. Det oppnådde produkt ble bearbeidet med en EVA-polymer (Escorene Ultra UL 02 02 0, Exxon), til en compound på et énskrueapparat, slik at compounden inneholdt 35% EVA-polymer og 65% modifisert aluminiumhydroksyd. In the intensive mixer (fluid/refrigerator mixer combination), 10 kg of aluminum hydroxide Martinal OL 107 (from Martinswerk GmbH) with an average grain size of approx. 0.9 - 1.3 jxm and an average specific surface according to BET of 6 - 8 m<2>/g mixed with 100 g (1.0% by weight) of an organopolysiloxane (SFR 100, General Electric Silicones) and 300 g (3.0 wt%) liquid EPDM with dicyclopentadiene (DCPD) as thermonomer and with an average molecular weight of 7000 (Trilene 65, Uniroyal) and 200 g (2 wt%) aminosilane (A 1100, Union Carbide) for a total of 10 minutes with a final temperature of 50 to 70°C. The product obtained was processed with an EVA polymer (Escorene Ultra UL 02 02 0, Exxon) into a compound on a single-screw apparatus, so that the compound contained 35% EVA polymer and 65% modified aluminum hydroxide.
Claims (8)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH395189 | 1989-11-01 |
Publications (3)
| Publication Number | Publication Date |
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| NO904734D0 NO904734D0 (en) | 1990-10-31 |
| NO904734L NO904734L (en) | 1991-05-02 |
| NO300850B1 true NO300850B1 (en) | 1997-08-04 |
Family
ID=4266988
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO904734A NO300850B1 (en) | 1989-11-01 | 1990-10-31 | Surface-modified magnesium hydroxide or aluminum hydroxide particles, their use, and highly combustible thermoplastic polyolefin |
Country Status (18)
| Country | Link |
|---|---|
| US (1) | US5139875A (en) |
| EP (1) | EP0426196B1 (en) |
| JP (1) | JP3023416B2 (en) |
| KR (1) | KR0174268B1 (en) |
| AT (1) | ATE101865T1 (en) |
| CA (1) | CA2028969C (en) |
| CZ (2) | CZ285219B6 (en) |
| DE (1) | DE59004678D1 (en) |
| DK (1) | DK0426196T3 (en) |
| ES (1) | ES2049388T3 (en) |
| FI (1) | FI103345B (en) |
| HU (1) | HU209676B (en) |
| IE (1) | IE64663B1 (en) |
| IL (1) | IL96162A (en) |
| MX (1) | MX172701B (en) |
| NO (1) | NO300850B1 (en) |
| RU (1) | RU2076118C1 (en) |
| ZA (1) | ZA908680B (en) |
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- 1990-10-24 IE IE383390A patent/IE64663B1/en not_active IP Right Cessation
- 1990-10-29 IL IL9616290A patent/IL96162A/en not_active IP Right Cessation
- 1990-10-30 ZA ZA908680A patent/ZA908680B/en unknown
- 1990-10-31 HU HU906968A patent/HU209676B/en not_active IP Right Cessation
- 1990-10-31 RU SU904831400A patent/RU2076118C1/en active
- 1990-10-31 NO NO904734A patent/NO300850B1/en not_active IP Right Cessation
- 1990-10-31 MX MX023137A patent/MX172701B/en unknown
- 1990-10-31 CA CA002028969A patent/CA2028969C/en not_active Expired - Fee Related
- 1990-11-01 JP JP2293781A patent/JP3023416B2/en not_active Expired - Fee Related
- 1990-11-01 CZ CS905376A patent/CZ285219B6/en not_active IP Right Cessation
- 1990-11-01 KR KR1019900017688A patent/KR0174268B1/en not_active IP Right Cessation
- 1990-11-01 US US07/607,686 patent/US5139875A/en not_active Expired - Fee Related
- 1990-11-01 CZ CZ972596A patent/CZ259697A3/en not_active IP Right Cessation
- 1990-11-01 FI FI905415A patent/FI103345B/en not_active IP Right Cessation
- 1990-11-02 EP EP90121055A patent/EP0426196B1/en not_active Expired - Lifetime
- 1990-11-02 AT AT90121055T patent/ATE101865T1/en not_active IP Right Cessation
- 1990-11-02 DE DE90121055T patent/DE59004678D1/en not_active Expired - Fee Related
- 1990-11-02 DK DK90121055.9T patent/DK0426196T3/en not_active Application Discontinuation
- 1990-11-02 ES ES90121055T patent/ES2049388T3/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JP3023416B2 (en) | 2000-03-21 |
| US5139875A (en) | 1992-08-18 |
| IL96162A0 (en) | 1991-07-18 |
| CZ285276B6 (en) | 1999-06-16 |
| NO904734L (en) | 1991-05-02 |
| JPH03263440A (en) | 1991-11-22 |
| DE59004678D1 (en) | 1994-03-31 |
| HUT55430A (en) | 1991-05-28 |
| ES2049388T3 (en) | 1994-04-16 |
| EP0426196B1 (en) | 1994-02-23 |
| CA2028969A1 (en) | 1991-05-02 |
| CZ537690A3 (en) | 1999-06-16 |
| IL96162A (en) | 1995-01-24 |
| MX172701B (en) | 1994-01-07 |
| EP0426196A1 (en) | 1991-05-08 |
| CZ259697A3 (en) | 1999-06-16 |
| FI103345B1 (en) | 1999-06-15 |
| ATE101865T1 (en) | 1994-03-15 |
| FI905415A0 (en) | 1990-11-01 |
| IE903833A1 (en) | 1991-05-08 |
| KR910009807A (en) | 1991-06-28 |
| IE64663B1 (en) | 1995-08-23 |
| CA2028969C (en) | 2002-05-28 |
| CZ285219B6 (en) | 1999-06-16 |
| ZA908680B (en) | 1991-10-30 |
| HU209676B (en) | 1994-10-28 |
| NO904734D0 (en) | 1990-10-31 |
| KR0174268B1 (en) | 1999-04-01 |
| FI103345B (en) | 1999-06-15 |
| RU2076118C1 (en) | 1997-03-27 |
| DK0426196T3 (en) | 1994-03-28 |
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